Dimethylformamide → 1-[(S)-4-(4-Chloro-2-fluoro-5-methoxy-phenyl)-2-methyl-piperazin-1-yl]-2-(3-iodo-pyrazolo[3,4-b]pyridin-1-yl)-ethanone

関与物質

役割	名称	HCID	仕込み量
反応物	Dimethylformamide	HCID 6228	—
反応物	Potassium Carbonate	HCID 11430	—
反応物	2-Chloro-1-[(S)-4-(4-chloro-2-fluoro-5-methoxy-phenyl)-2-methyl-piperazin-1-yl]-ethanone	HCID 57642767	—
反応物	HCID 178506575	HCID 178506575	—
溶媒	Ethyl Acetate	HCID 8857	—
生成物	1-[(S)-4-(4-Chloro-2-fluoro-5-methoxy-phenyl)-2-methyl-piperazin-1-yl]-2-(3-iodo-pyrazolo[3,4-b]pyridin-1-yl)-ethanone	HCID 16006032	99.2%

反応条件

温度	90 °C

反応手順

A mixture of 2-Chloro-1-[(S)-4-(4-chloro-2-fluoro-5-methoxy-phenyl)-2-methyl-piperazin-1-yl]-ethanone (1.37 g, 4.08 mmol, 1 eq), 3-Iodo-1H-pyrazolo[3,4-b]pyridine (1.0 g, 4.08 mmol, 1 eq), potassium carbonate (2.26 g, 16.4 mmol, 4 eq), and DMF (15 ml) was stirred overnight at 90° C. The reaction solution was diluted with ethyl acetate, washed with saturated aqueous NaHCO3, and concentrated in vacuo. The crude product was purified by flash chromatography to provide 1-[(S)-4-(4-Chloro-2-fluoro-5-methoxy-phenyl)-2-methyl-piperazin-1-yl]-2-(3-iodo-pyrazolo[3,4-b]pyridin-1-yl)-ethanone (2.2 g).

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08383630B2
出典データセット	uspto-grants-2013_02
ORD ID	ord-996386de161a4f668ebc642c1b0eb01b
出典メモ	uspto-grants-2013_02